Aspen Plus Simulation

World Academy of Science, Engineering and Technology
International Journal of Chemical and Molecular Engineering

Vol:8, No:10, 2014
Aspen Plus Simulation of Saponification of Ethyl

Acetate in the Presence of Sodium Hydroxide in a
Plug Flow Reactor
U. P. L. Wijayarathne, K. C. Wasalathilake
main factors which affects the choice of diameter. PFRs are

Abstract—This work presents the modelling and simulation of widely used in the industry for gas and liquid phase systems.
saponification of ethyl acetate in the presence of sodium hydroxide in Gasoline Production, Oil cracking, oxidation of sulfur dioxide
a plug flow reactor using Aspen Plus simulation software. Plug flow to sulfur trioxide, synthesis of ammonia, polymer
reactors are widely used in the industry due to the non-mixing manufacturing are some the industries where PFRs are being
property. The use of plug flow reactors becomes significant when
there is a need for continuous large scale reaction or fast reaction. used broadly.
Though they are a number of applications, the controlling of
Open Science Index, Chemical and Molecular Engineering Vol:8, No:10, 2014 waset.org/Publication/9999474
Plug flow reactors have a high volumetric unit conversion as the

occurrence for side reactions is minimum. In this research Aspen Plus PFR has become a challenging task when it comes to chemical
V8.0 has been successfully used to simulate the plug flow reactor. In manufacturing. Time varying characteristics of the process
order to simulate the process as accurately as possible HYSYS Peng- have made the operation of the reactor difficult and it needs
Robinson EOS package was used as the property method. The results extensive monitoring. For overcome such issues, modelling
obtained from the simulation were verified by the experiment carried
out in the EDIBON plug flow reactor module. The correlation and simulation of reactors has become useful when it comes to
coefficient (r2) was 0.98 and it proved that simulation results process optimization and to investigate the effect of various
satisfactorily fit for the experimental model. The developed model operating parameters towards the process.
can be used as a guide for understanding the reaction kinetics of a Practice of process simulation has evolved over last two
plug flow reactor. decades in the field of engineering. When it comes to process
engineering, there is a wide range of process simulation
Keywords—Aspen Plus, Modelling, Plug Flow Reactor, packages which are specifically developed for particular
Simulation.
process areas namely, Aspen Plus, Chemcad and Petro-SIM.
All these simulators follow the sequential modular approach
I. INTRODUCTION
where the user is able develop a process by combining
P LUG flow reactors (PFRs) also known as Continuous

Tubular Reactors (CTRs) play a key role in chemical
manufacturing facilities where a transformation of chemical
standard modules in a logical manner. Aspen Plus is one of the
industry’s leading process simulation software which has the
ability to design and simulate a chemical process
substances takes place. In a plug flow reactor, feed is comprehensively.
introduced from one end of a cylindrical tube and flows Aspen Plus has been used by investigators to simulate and
continuously through the length of the reactor as a series of optimize various kinds of process plants and unit operations.
plugs. The product is then collected from the other end of the Sohail Rasool Lone et al. developed a model to simulate ethyl
reactor. In modelling it is assumed that Inside a PFR, the acetate reactive distillation column using a RADFRAC model
fluids flow consistently and there is no radial variation in [2]. Harjeet Nath et al. developed a model to simulate the
velocity, concentration, temperature, or reaction rate [1]. The abatement of fluorine inside a fluidized bed reactor using
main advantages of PFRs are that they have a high volumetric RCSTR and RGIBBS models [3]. Rajul Nayak et al.
unit conversion and the capability of running for longer developed a model to simulate coal gasification using
periods without maintenance. For isothermal reactions greater RYIELD, RGIBBS and RSTOIC models [4].
than zeroth order, the PFR volume will usually be lower than The primary objective of this study is to develop a model
the Continuously Stirred Tank Reactor (CSTR) volume for the for a Plug Flow Reactor and to simulate the saponification of
same conversion and reaction conditions (temperature, flow ethyl acetate in the presence of sodium hydroxide by varying
rate, etc.) [1]. the reactor temperature and reactant flow rates using Aspen
For the industry, PFR can be configured as a single long Plus. In order to validate the applicability of the developed
tube or a bunch of short tubes depending on the application. model, simulation results were compared with the
The diameter of the cylindrical reactor varies from a few experimental results collected using EDIBON PFR module
centimeters to several meters. Construction cost, pumping [5]. During the laboratory experiment, fractional conversions
cost, residence time and heat transfer requirements are the of the reaction are determined using the conductivity values of
the reactants and products under different temperatures.
Wijayarathne U.P.L and Wasalathilake K.C. are with the Department of
Chemical & Process Engineering, University of Moratuwa, Sri Lanka (e-mail:
udithaw@uom.lk and kimalw@uom.lk, respectively).
International Scholarly and Scientific Research & Innovation 8(10) 2014 1089 ISNI:0000000091950263
Vol:8, No:10, 2014
II. NOMENCLATURE the products CH! COO/ Na0 C" H# OH as well as the unreacted
T - Absolute Temperature NaOH, conductivity of the product stream could be expressed
C - Concentration as, [8]
x - Fractional Conversion
k - Frequency Factor κ123&456 'λ() * C() + 'λ,-. * C,-. + 7λ8-98,,. * C8-98,,. : (5)
λ - Molar Conductivity of an ion
k - Rate Constant Furthermore, online conductivity meter displays the
r - Rate of Reaction conductivity value for the solution as at 25oC. Therefore, it
v - Reactor Volume should be corrected to the operating temperature using the
expression, [9]
T
- Reference Temperature
κ - Solution Conductivity ;
κ
- Solution Conductivity at T
κ
;0</ * κ (6)
=>?>=>@A>
- Temperature Coefficient
R - Universal Gas Constant Hydrolysis reaction of ethyl acetate with sodium hydroxide
F - Volumetric Flow Rate is in the form of A B C D. Moreover, the concentration
of both the NaOH and CH! COOC" H# are similar, the
III. THEORY concentration of components at initially and any time t, can be
expressed as follows.
A. Saponification
Saponification is the hydrolysis of a carboxylic acid ester in TABLE I
a basic medium (1). Saponification is essentially a soap- CONCENTRATION OF STREAMS WITH TIME
manufacturing process that takes place by reacting the fatty Time EF EG EF EG
acid with alkali, especially triglycerides producing glycerol t=0 EFH EFH 0 0
EFH 1 JF EFH 1 JF EFH JF EFH JF
and carboxylate salts (soap). t=t
2 2 2 2

NaOH CH3 COOR CH3 COO Na ROH (1)
By replacing the concentration terms in above (4) and (5),
In this experiment, saponification of ethyl acetate in the
presence of sodium hydroxide is used to demonstrate the
κ$%%& 7λ() * EFH : 7λ,-. * EFH :
saponification reaction. The saponification of ethyl acetate
and
reaction is as follows. LMH ;/NM LMH NM
κ123&456 7λ() * EFH : Kλ,-. * "
O Kλ8-98,,. *
"
O.

NaOH CH3 COOC2 H5 CH3 COO Na C2 H5 OH (2)
Fractional conversion could be determined by solving for x.
when it comes to chemical kinetics, this reaction is a C. PFR Theory
prominent second order reaction identified in literature [6],
[7]. Since the saponification of ethyl acetate with presence of
sodium hydroxide is a second order reaction [6], rate of the
In a PFR, reactant fluids are pumped through a tubular
reaction can be expressed as follows.
section where the reaction is carried out. At the inlet of the
PFR, reactant concentration is very high, hence the rate of
r kC(,- C8-98,,8Q -R (7)
reaction is also high. But, when it passes through the reactor,
reactants get consumed and products are formed. Therefore
According to the Arrhenius equation
rate of reaction drops through the PFR with respect to reactor
length. /W
k k exp V Y (8)
X
B. Conductivity Theory
Conductivity of a solution is given by, κ λm C(3) [8]. Tubular reactors falls under the category of flow reactors
Where, λ is the molar conductivity of an ion and C is the ion where the key assumption is that the fluid is perfectly mixed in
concentration in the solution. Feed stream for the PFR consists the radial direction but not in the axial direction (zero back
with equal volumetric flow rates of NaOH and mix). Each plug of differential volume is considered as a batch
CH! COOC" H# . Since the conductivity value for
reactor where the volume tends to be zero.
The PFR model is well applied for many fluids. Ideal PFR
CH! COOC" H# is negligible with reference to NaOH ,
consist with a constant residence time which is same as the
conductivity of the feed solution can be estimated as, [8] space time if other conditions such as pressure and
temperature are same throughout the reactor [10]-[12].
κ$%%& 'λ() * C() + 'λ,-. * C,-. + (4)
D.Plug Flow Reactor Design Equation
Similarly for the product stream, since it consists with both General assumptions made for mathematically model an
Vol:8, No:10, 2014
ideal plug flow reactor, to the tubular section where the reaction is carried out
• There is no mixing in the axial direction (direction of • Tubular section is having a diameter of 5.8mm and a
flow) length of 16.5m
• Complete mixing in the radial direction • Type “J” temperature sensor to get the temperature of the
• Uniform velocity profile across the radius reactor in a continuous way
• An online conductivity meter (CRISON CM38)
• Three Pyrex-glass tanks of 10 liters capacity, two of them
for the reagents and the other one for the accumulation of
product.
2. Conductivity Monitoring Instrument
CRISON CM38, an online conductivity and temperature
Fig. 1 Elemental material balance for a PFR meter available with EDIBON PFR module was used to
measure the conductivity and the temperature of the product
Applying material balance for component A (NaOH) over stream. According to the product specifications, this online
small elemental volume dv under the steady state operation device is capable of measuring the conductivity of a solution
results, in the range of 0.01 µS/cm to 199.9 mS/cm with error
percentage ≤ 1% and also it is capable of measuring the
CZ 1 x F rF dv CZ 1 x dx F 0 temperature of a solution in the range of -20oC to 150oC with
rF dv CZ Fdx error ≤ 0.5°C. Reference temperature for the measuring device
_ c bc
CZ a (9) is 25°C and all the conductivity values display as at reference
` /M
temperature [13].
Residence time is same as the space time and given by
_
τ (10)
`
Therefore,
c bc
τ CZ a (11)
e8fH Q ;/c Q
IV. METHODOLOGY
A. Materials
All chemicals used for this work are of analytical reagent
grade. The stock solutions of NaOH (∼0.1 M) and ethyl
Fig. 2 PFR and Conductivity meter
acetate (∼0.1 M) were prepared using distilled water. Ethyl
acetate from Sigma-Aldrich Corporation, Spruce St., St. C. Method
Louis, Missouri United States with 99% assay (density: 0.902 10 liter of 0.1M NaOH and 0.1M CH3COOC2H5 (ethyl
g cm−3) was directly used as stock solution. 99.8% assay acetate) solutions were prepared and stored in feed vessels.
NaOH pellets from Merck Specialties Private Limited, Plug Flow Reactor module was switched on and the water
Mumbai, India was used and the stock solution of NaOH was bath temperature was set to 30°C. Circulation pump was
standardized against freshly prepared standard hydro chloric switched on in order to circulate the hot water to the shell side
acid. of the PFR. Flow rate of 0.1M NaOH was set to 2.4 l/h and
B. Experimental Setup allowed the system to reach steady state. Once the
conductivity value was stable, it was recorded from the online
1. Reactor Module conductivity meter. Water bath temperature was gradually
Plug Flow Reactor in EDIBON Computer Controlled increased to 35°C, 40°C and 45°C while maintaining the flow
Chemical Reactors Training System was used to carry out the rate of NaOH solution at 2.4l/h. Conductivity values
hydrolysis reaction. The experimental setup was mainly corresponding to these temperatures were recorded for latter
equipped with following components. calculation requirements. Then the PFR was thoroughly
• Two computer controlled feed pumps coupled with flow washed using distilled water while allowing the water bath to
meters to measure the flow of liquids in the range of 0.7-7 cool down.
l/h and 0.54-5.4 l/h Once the temperature of the PFR reached to 30°C, flow
• Thermostatic bath of 9 liters capacity that regulates the rates of NaOH& ethyl acetate was set as 2.4 l/h and both the
temperature between ambient temperature and 70oC with feed pumps were switched on simultaneously to feed the
a level switch and a pump which are computer controlled reactants to PFR.
• An online feed pre-heater prior to introduce the reactants Hydrolysis reaction was carried out inside the PFR
Vol:8, No:10, 2014
according to the reaction (2). ESTER PRODUCT
System was allowed to reach steady state operation and the FEED
NAOH
conductivity of the product stream was recorded using the MIXER
online
line conductivity meter. Water bath temperature was again PFR
gradually increased to 35°C, 40°C C and 45 45°C while Fig. 3 Aspen Flow Sheet
maintaining the flow rates of the reactants at 2.4 l/h.
Conductivity values of the product stream corresponding to
these temperatures were also recorded.
Fractional conversion for the reaction (2) was calculated
using the conductivity values recorded from the product
stream at different temperatures. These results were compared
with the simulation results from Aspen Plus V8.0.
D.Method Aspen Simulation
PFR
FR was modeled in Aspen Plus according to the
dimensions and the operating conditions of the EDIBON
reactor module. Then it was compared with the experimental
results. HYSPR was used as the property method for the
Aspen model. Fig. 4 PFR Configuration

roperty methods available in
There are various physical property
Aspen Plus V8.0 which can be used for the estimation of
physical properties. HYSPR (HYSYS Peng-Robinson
Peng EOS
package) property model was used in this study [14].
Two inbuilt models of a Mixer and a PFR were used to
model the system (Fig. 3). In the experimental setup two
reactants were mixed together before introducing to the PFR.
Therefore a model of a Mixer was used in the aspen
simulation to represent this operation. Two feed streams, Ethyl
acetate and Sodium hydroxide were defined fined as ESTER and
NAOH respectively. Concentration of the feed solutions were
set as 0.1 mol/dm3 where, the solvent was defined as water
since both the reactants were in aqueous medium and the flow
rate for each feed was set as 2.4 l/h. Temperature and pressure
pr
for feed streams were set as 30oC and 1 atm respectively.
PFR model in the aspen simulation represent the tubular Fig. 5 PFR Reaction Kinetics Data
reactor in the experimental module and the parameters were
set accordingly. Length of the reactor was 16.5m and the V. RESULTS AND DISCUSSION
diameter of the tubee was 5.8mm. Phase of operation for the A. Conductivity
vity vs. Temperature
experimental model was only liquid and therefore valid phase
40
the PFR model in the Aspen was selected as liquidliquid- only (Fig.
Conductivity (mS/cm)
4). Operating condition for the PFR was set as 30oC and 1atm. 30
After setting up the physical parameters, reaction kinetic
parameters were introduced to the Aspen model. According to 20 k0
(mS/cm)
the literature [8], the saponification reaction follows the power 10
law (7) and hence it was selected as the reaction class in the
Aspen model. Driving force was also sett as ‘exponent’ of one 0
for both the reactants since the reaction rate is proportional to 30 35 40 45
Temperature (oC)
the concentration of each of the reactant. Activation energy
(Ea) and frequency factor (h ) were found to be 41400 Fig. 6 Solution Conductivity vs. Temperature
kJ/kmol and 2194760 respectively [8] 8] and those vvalues were
fed to the Aspen model (Fig. 5). The results that were obtained Conductivity values of both NaOH stream and product
upon the simulation off the model are given in Table IIIIII. stream were adjusted to the operating temperature of the
reactor according to (6) and were plotted against the reactor
temperature (Fig. 6). The conductivity values of the solution
show linear dependence on the reactor temperature.
Vol:8, No:10, 2014
B. Comparison of Simulated Results and Experimental C. Effect of Temperature on the Reaction

Results TABLE II
FRACTIONAL CONVERSION AT DIFFERENT REACTOR TEMPERATURES
Table II shows the calculated results for the fractional
Reactor Temperature (oC) 30 35 40 45
conversion of the saponification reaction at different reactor
Experimental results 0.73 0.76 0.80 0.83
temperatures for both the experiment and the simulation. It is
Simulated results 0.72 0.77 0.81 0.84
clear from the results that in both the cases, the fractional
conversion increases as the reactor temperature increases.
The experimental values obtained for fractional conversion
conver Figs. 8-11
11 show the variation of molar fractions of ethyl
were correlated with the results obtained from the simulation acetate and sodium acetate at the reactor temperatures of
(Fig. 7). The correlation coefficient (r2) was 0.98 and it proved 30°C, 35°C, 40°C and 45°C respectively. It is clear from these
that simulation results show a good fit for the experimental figures that the molar fractions of reactants decrease with the
model. increment of reactor temperature. This is due to the fact that
the reaction rate increases with the reactor temperature and
hence, the molar fractions of products increase (7&8).
Fig. 13 shows the curve for molar flow of sodium acetate
obtained under different reactor temperatures (From 25°C 25 to
200°C . It can be seen that the sodium acetate molar flow rate
increases with the reactor temperature and it reaches a
maximum value of 0.24 mol/h when the reactor temperature

is150°C.
It is also evident that the molar fractions of products
increase with increment
ment of length of the plug flow reactor.
This is because the residence time of reactants increases with
the length of the reactor, where it allows sufficient time for the
reaction to take place (11).
Fig. 7 Fractional conversion vs. reactor temperature
TABLE III
RESULTS SUMMARY
Caustic Ester Product Product Product Product
at 30oC at 35oC at 40oC at 45oC
H" O kmol/h 1.7055E-01 1.6950E-01 3.4005E-01 3.4005E-01 3.4005E-01
3.4005E 3.4005E-01
CH! COOC" H# kmol/h - 2.4000E-04 6.6052E-05 5.4319E-05 4.5229E-05
4.5229E 3.7255E-05
NaOH kmol/h 2.4000E-04 - 6.6052E-05 5.4319E-05 4.5229E-05
4.5229E 3.7255E-05
CH! COO/ Na0 kmol/h - - 1.7395E-04 1.8568E-04 1.9477E-04
1.9477E 2.0275E-04
C" H# OH kmol/h - - 1.7395E-04 1.8568E-04 1.9477E-04
1.9477E 2.0275E-04
Total Flow kmol/h 1.7079E-01 1.6974E-01 3.4053E-01 3.4053E-01 3.4053E-01
3.4053E 3.4053E-01
Total Flow kg/h 3.08 3.07 6.16 6.16 6.16 6.16
Total Flow l/min 0.04 0.04 0.08 0.08 0.08 0.08
Fig. 8 Ethyl acetate mole fraction vs. PFR length at 30°C
Vol:8, No:10, 2014

35

45
Vol:8, No:10, 2014
Fig. 12 Variation of ethyl acetate mole fraction with acetate and NaOH flow rates
product stream. Therefore though same amount of sodium

acetate is produced by the reaction, mole fraction of sodium
acetate is decreased because of the presence of unreacted ethyl

acetate
etate in the product stream.
E. Volume Comparison of CSTR and PFR
Volume required for a PFR is relatively less when
compared to the volume required for a Continuous Stirred
Tank Reactor (CSTR) to achieve the same conversion for a
reaction while maintaining thet other parameters as constant
[15]. This theory is well applied for the saponification reaction
Fig. 13 Variation of sodium acetate flow rate with reacto
reactor of ethyl acetate with sodium hydroxide. During this study it
temperature
has also proven with using Aspen simulation that the volume
of CSTR to achieve the same conversion
conversio is about 3.5 times
that of a PFR (Fig. 14). Therefore, it is economically feasible
to use a PFR to carry out this saponification reaction in
industrial scale even when producing with large quantities.
VI. CONCLUSION
In this work, a simulation model was developed
devel for the
reaction of saponification of ethyl acetate in the presence of
sodium hydroxide inside a plug flow reactor using Aspen Plus.
The model was validated by the experimental results obtained
from EDIBON Plug Flow Reactor module. The experimental
results
sults showed a good fit to the Aspen Plus model.
Fig. 14 Ethyl acetate mole fraction vs. reactor volume Aspen Plus model proved that the rate of reaction increases
as the reactor temperature and the length of the plug flow
D.Effect of Reactant Flow Rates on the Reaction
reactor increase. The highest yield of the reaction was
A sensitivity analysis was done in Aspen Plus model to obtained at a reactor temperature
temperatu of 150°C.
investigate the effect of reactant flow rates towards the These results improve the understanding of reaction kinetics
reaction. with reference to the saponification reaction and would be
Fig. 12 shows how the mole fractions of sodium acetate very useful in the design of plug flow reactors.
vary for different flow rates of NaOH and ethyl acetate. It
shows that in each case the highest mole fraction of sodium ACKNOWLEDGEMENTS
acetate can be achieved when equal flow rates of NaOH and
ethyl acetate are pumped to the plug flow reactor. According The authors would like to acknowledge Dr. Ismail F. M.,Dr.
M.,Dr
to the stoichiometry of (2) it is clear that equal amounts of Gunasekera M. Y. and Mr. Rathnayake H.H.M.P. for
reactants are needed to obtain the highest yield. providing the space and all facilities needed in the research
When the flow rate of ethyl acetate exceeds the flow rate of study at the Department of Chemical and Process Engineering,
NaOH as there is no more NaOH left in the rea reactor to react University of Moratuwa, Sri Lanka.
with ethyl acetate, the excess ethyl acetate remains in the
Vol:8, No:10, 2014
REFERENCES
[1] Fogler, H. Scott. Elements of Chemical Reaction Engineering. : Prentice
Hall Professional Technical Reference, 2006. ISBN 23-13-047394-4 .
[2] Modeling and Simulation of Ethyl Acetate Reactive Distillation Column
Using Aspen Plus. Ahmad, SohailRasool Lone & Syed Akhlaq. Issue 8,:
International Journal Of Scientific & Engineering Research, 2012, Vol.
Volume 3. ISSN 2229-5518.
[3] Abatement of Fluorine inside a Fluidized Bed Reactor Using Aspen Plus
Simulation. Sahoo, HarjeetNath and Abanti. Odisha : International
Conference on Frontiers in Chemical Engineering, 2013.
[4] Simulation of Coal Gasification Process using ASPEN PLUS.
Ahmedabad: International Conference on Current Trends in Technology,
2011.
[5] Equipment, Edibon Technical Teaching. Computer Controlled Chemical
Reactors Training System with SCADA and PID Control. Madrid:
Edibon International, 2013.
[6] Walker, J. A Method for Determining Velocities of Saponification:
Royal Society of London, 1906.
[7] Carl Garland, Joseph Nibler , David Shoemaker. Experiments in
Physical Chemistry. : McGraw-Hill, 2003.
[8] Peter Atkins, Julio de Paula. Atkins' Physical Chemistry. Eighth Edition.
New York: Oxford University Press, 2006. ISBN: 0-7167-8759-8.
[9] Analytical, Radiometer. Conductivity Theory and Practice. France :

Radiometer Analytical SAS, 2004.
[10] Denbihh, K. G., and J. C. R. Turner, Chemical Reactor Theory, 2nd
edition, Cambridge University, 1971
[11] Levenspiel, O., Chemical Reaction Engineering, 2nd edition, John Wiley
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[12] Smith, J. M., Chemical Engineering Kinetics, 3rd edition, McGraw-Hill,
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[13] CRISON Instruments, S.A. Controladores CM38-CM38P Manual del
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[15] Wittrup, Prof. K. Dane. Chemical and Biological Reaction Engineering,
Spring 2007. ocw.mit.edu. (Online) 2007. (Cited: 05 30, 2014.)

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World Academy of Science, Engineering and Technology

International Journal of Chemical and Molecular Engineering

Aspen Plus Simulation of Saponification of Ethyl

main factors which affects the choice of diameter. PFRs are

Plug flow reactors have a high volumetric unit conversion as the

P LUG flow reactors (PFRs) also known as Continuous

according to the reaction (2). ESTER PRODUCT

Aspen model. Fig. 4 PFR Configuration

B. Comparison of Simulated Results and Experimental C. Effect of Temperature on the Reaction

maximum value of 0.24 mol/h when the reactor temperature

Fig. 8 Ethyl acetate mole fraction vs. PFR length at 30°C

Fig. 9 Ethyl acetate mole fraction vs. PFR length at 35°C

Fig. 10 Ethyl acetate mole fraction vs. PFR length at 40°C

Fig. 11 Ethyl acetate mole fraction vs. PFR length at 45°C

product stream. Therefore though same amount of sodium

acetate is decreased because of the presence of unreacted ethyl

[9] Analytical, Radiometer. Conductivity Theory and Practice. France :

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